反应 #156823

ord-c0499d0168ab4fbd9bfe9ee366c17ebb

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The viscous yellow reaction
  2. 2
    温度was heated to 90° C. for one hour
  3. 3
    温度to cool back to room temperature
  4. 4
    其他purified

实验过程

Methyl 6-chloro-5-nitronicotinate (2.0 g, 9.23 mmol) was added to methyl 2-(methylamino)acetate (1.9 g, 18.47 mmol) neat while stirring at room temperature. The viscous yellow reaction was heated to 90° C. for one hour and then allowed to cool back to room temperature. The reaction was diluted with dichloromethane (20 mL) and purified using flash column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes) to yield 2.60 g (99% yield) of the title compound as a yellow oil. [M+H] calc'd for C11H13N3O6, 284; found, 284.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08822470B2uspto-grants-2014_09